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MOFs as catalysts for ring-opening polymerization

A polymerization catalyst, a technology of ring-opening polymerization, applied in the field of lactide polymerization, can solve problems such as low activity

Inactive Publication Date: 2020-12-29
夏玲
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, compared with a large number of other organic reactions, until now there have been no studies on 3D MOFs for heterogeneous ring-opening polymerization catalysis
The most closely related report comes from Chuck (Chuck C.J., Davidson M.G., Jones M.D., Kociok-G., Lunn M.D., Wu S. Inorg. Chem. 2006, 45, 6595-6597.), which reported that in ε- Use of three-dimensional titanium-based materials as initiators in the controlled ring-opening polymerization of caprolactone and lactide, and from the Lin research group (C.-Y.Wu, D.S.Raja, C.-C.Yang, C. -T.Yeh, Y.-R.Chen, C.-Y.Li, B.-T.Ko, C.-H.Lin CrystEngComm 2014, 16, 9308-9319.), who found that 2D zinc inorganic polymer Can initiate ring-opening polymerization of L-lactide, but its activity is much lower than previously reported Ti catalysts

Method used

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Experimental program
Comparison scheme
Effect test

Embodiment

[0049] Catalyst preparation

[0050] All 3D MOFs catalysts were prepared using a solvothermal method, modifying the synthetic procedures according to those described in ref.

Embodiment I

[0052] Synthesis of ZnDABCO and CoDABCO

[0053] In a typical ZnDABCO synthesis process, Zn(NO 3 ) 2 ·6H 2 O (5.4mmol, 1610mg) was mixed with BDC (5mmol, 830mg) and DABCO (2.5mmol, 280mg) in 60ml DMF, then transferred to a Teflon-lined autoclave and heated at 120°C for 48h. After that, the mixture was cooled to room temperature. The white solid product was filtered and washed three times with DMF, then dried under vacuum at room temperature (25-30° C.) overnight. The dried material was transferred to a vacuum desiccator for storage.

[0054] The synthesis process of CoDABCO is similar to that of ZnDABCO. Therefore, the Co(NO 3 ) 2 ·6H 2 O (3mmol, 873mg), BDC (3mmol, 498mg) and DABCO (2.5mmol, 280mg) were mixed in 60ml DMF and transferred to a Teflon-lined autoclave which was heated at 120°C for 48h.

[0055] (S. Chaemchuen, K. Zhou, N. Alam Kabir, Y. Chen, X. Ke, G. Van Tendeloo, F. Verpoort Micropor. Mesopor. Mater. 2015, 201, 277-285.)

Embodiment II

[0057] Synthesis of ZnBDC

[0058] In 10mL DMF from Zn(NO 3 ) 2 ·6H 2 A mixture of O (1.48mmol, 440mg) and BDC (1.12mmol, 185mg) was used to synthesize MOF-5, and a small amount of water (180μL) was added. The mixture was then transferred to a Teflon-lined autoclave and heated at 120 °C for 48 h. The autoclave was then cooled to room temperature. The resulting white solid was washed with DMF and dried in an oven at 150 °C for 12 h. Store the dried product in a desiccator.

[0059] (B. Chen, X. Wang, Q. Zhang, X. Xi, J. Cai, H. Qi, S. Shi, J. Wang, D. Yuan, M. Fang J. Mater. Chem. 2010, 20, 3758-3767.)

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Abstract

The present invention provides a process for the ring opening polymerization of lactide in the absence of solvent, and with metal-organic frameworks (MOFs) as catalysts.

Description

[0001] field of invention [0002] The present invention relates to a process for the polymerization of lactide (L-, D-, meso- and mixtures thereof) catalyzed by three-dimensional metal-organic frameworks (MOFs) materials. [0003] Background of the invention [0004] Polylactic acids (PLAs) have been considered as promising alternatives to traditional industrial polymers due to their outstanding properties, such as biosolubility, biodegradability, and biocompatibility. Ring-opening polymerization (ROP) is an excellent method for the synthesis of high molecular weight polylactic acid with homogeneous organometallic or Lewis acid catalysts. [0005] However, impurities in the polymer from homogeneous catalysts can limit the practical application of previously prepared polymer products. It is desirable to use recyclable solid catalysts to allow easy separation of the catalyst from the polymer produced to remove catalyst residues. However, there are only a few publications repor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G63/08C08G63/06C08G63/83C08G63/84C08G63/85
CPCC08G63/08C08G63/823C08G63/88
Inventor 弗朗西斯·沃尔特·科尼利厄斯·维尔波特罗志雄
Owner 夏玲
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